Liquid Extraction Method Research Articles

Comparison of extraction process, physicochemical properties, and in vitro digestion characteristics of chia seed mucilage polysaccharide.

The study explored five (acidic, alkaline, heating, ionic liquid, and urea solvent) extraction methods' effects on chia seed mucilage polysaccharide (CSM), an anionic polymeric macromolecule, regarding its physicochemical properties, structure, and digestion behavior. The results showed that extraction parameters have a considerable effect on modulating CSM properties. Significant differences emerged in the predominant chemical compositions: the carbohydrates and protein content ranged from 49.20±0.06% to 85.81±0.03%, and 3.20±0.13% to 14.57±0.30%, respectively. The structural analysis revealed that alkaline heating treatment facilitated the formation of protein-polysaccharide conjugates, resulting in reduced particle size, enhanced ζ-potential, and improved thermal stability (194.72±2.19J/g). The crystallinity of CSM varied, peaking at 42.9±0.22% without pH adjustment and heating. CSM extracted using 6M urea exhibited the lowest protein content, and crystallinity (25.50±0.09%), coupled with the highest gastrointestinal digestion rate and poorest thermal stability (with a carbohydrate degradability of 24.223±1.78% and enthalpy value of 62.82±0.32J/g). The CSM obtained under alkaline heating showed minute particles (201.1±10.35μm), the highest ζ-potential absolute value (20.95±2.28mV), and robust thermal stability (194.72±2.19J/g of enthalpy value), which is ideal for stabilizing emulsions or encapsulating thermolabile substances. Additionally, compared to monovalent cations‑sodium ions, divalent cations‑magnesium ions, is more tend to aggregate the CSM structure, resulting in larger molecular particles and a higher protein content. Elevated ionic concentration further diminished thermal stability. These findings suggest that CSM is a customizable, multi-purpose polymer that can be extracted in various ways based on the end-product requirements.

Synchronization of extraction and chromatographic conditions of diverse physicochemical behavior of pseudoephedrine, loratadine and desloratadine for their simultaneous determination in human plasma: Application to pharmacokinetic study

A selective, sensitive, and rapid LC-MS/MS method has been developed, optimized, and validated for the simultaneous determination of pseudoephedrine (PSE), loratadine (LOR), and LOR active metabolite, desloratadine (DES) in K3EDTA human plasma. A simple liquid–liquid extraction method was adopted for extraction of the 3 analytes and their internal standards; chlorpheniramine (CLP), loratadine D4 (LOR-D4), and desloratadine D4 (DES-D4), respectively, giving consistent recovery results (78.38––88.23 %) using diethyl ether: dichloromethane (80:20, v/v) as the extraction solvent. The chromatographic separation was challenging due to the polarity differences between PES, which is more polar, and LOR and DES, which are less polar that affected their physicochemical properties including the retention of the drugs on C18 column. The separation was achieved using of isocratic elution of 20 mM ammonium formate and 2 mM trifluoracetic acid ammonium salt: acetonitrile containing 0.15 % formic acid (12:88, v/v) as a mobile phase pumped onto a Supelco Discovery® C18 (4.6 mm x 100 mm, 5 µm) at 35 °C with a flow rate of 0.8 mL/min. The use of trifluoracetic acid ammonium salt as an ion pair reagent in the selected mobile phase allowed good retention of the polar PSE on the used C18 column with a reasonable retention time. Positive Electrospray ionization was employed followed by detection using a tandem mass spectrometer in multiple reactions monitoring (MRM) mode. The sample analysis of this study was conducted in compliance with ICH guideline M10 on bioanalytical method validation and study sample analysis. The method was linear over the concentration range of (4–1200) ng/mL for PSE, (50–15000) pg/mL for both LOR, and DES. The developed method was accurate (91.14–110.30 %), precise (0.53–7.86 %), and was applied to study the pharmacokinetic profile of the cited drugs in the plasma of healthy human volunteers after single oral administration of the fixed-dose combination Claritin D® tablet, (240/10 mg) of PSE, and LOR, respectively.

Three liquid phase membrane extraction method based on the electro-migration assisted by high-performance liquid chromatography for the analysis of carcinogenic heterocyclic aromatic amines in steak samples

A combination of microwave digestion and three-phase hollow fiber electromembrane extraction (HF-EME) with high-performance liquid chromatography (HPLC) was designed to determine carcinogenic heterocyclic aromatic amines (HAAs) in steak samples. The recorded fingers of merit (LOD: 1.4–1.6 ng/g, LOQ: 4.5–5.2 ng/g, RSD: 6.1–7.2 %, recovery: 91–95 % and EF: 107–112) underlines the adequacy of the proposed technique. The total of 2-amino-3-methylimidazo[4,5-f] quinoline (IQ), 2-amino-3,8-dimethylimidazo [4,5-f] quinoxaline (MeIQx), 2-amino-3,4 dimethylimidazo[4,5-f] quinoline (MeIQ) and 2-amino-1-methyl-6-phenylimidazo[4′5-b] pyridine (PhIP) in steak samples were 93.46 ± 4.93–174.52 ± 10.91 ng/g, 31.65 ± 1.87–877.97 ± 56.19 ng/g, 10.08 ± 1.01–535.73 ± 18.93 ng/g, and 62.56 ± 1.89–341.23 ± 41.45 ng/g, respectively. Lamb steak contain highest amount of MeIQx (877.97 ± 56.19 ng/g) and beef steak showed lowest concentration of MeIQ (10.08 ± 1.07 ng/g). In conclusion, several interesting features such as great recovery, suitable enrichment factor, very low sample amount and organic solvent requirement and short extraction time make this novel method appropriate for the analysis of the negligible levels of HAAs in complex food matrices.

Comprehensive targeted profiling of multiple steroid classes in rodent plasma using liquid chromatography-mass spectrometry

BackgroundReliable quantification of multiple steroid classes in biological fluids within a single method remains an analytical challenge despite many previously published methods. Crosstalk of positional isomers, overlap of stereoisomer fragmentation patterns, differing proton affinities, in-source fragmentation, varying stability of protonated ions in the gas phase across steroid classes, and non-existence of steroid-free matrix are the main challenges limiting the number of simultaneously profiled steroids. ResultsIn this study, we focused on the development of a derivatization-free, achiral, high-throughput, and cost-effective UHPLC-MS/MS approach that allows simultaneous profiling of a spectrum of 38 steroids covering progestogens, androgens, corticosteroids, and estrogens, while properly addressing the hurdles of steroid analysis. Within a 20-min method, 16 stereoisomers and 15 positional isomers were fully resolved within a single run while separated from 7 additional non-interfering steroids and matrix interferences in rodent plasma. Protein precipitation (PP) and supported liquid extraction (SLE) methods using only 40 μL of sample were developed to achieve the lowest possible limits of quantification. Nevertheless, 5α-dihydroprogesterone and 3α,5α-THDOC could be only qualitatively assessed when using PP. In contrast, DHEA-S could not be quantified or identified when using SLE. A novel surrogate matrix-background subtraction approach, using rat plasma after the animal's adrenalectomy, has been implemented into the optimized PP-UHPLC-MS/MS workflow, successfully validated according to the unified ICH/EMA M10 guidelines, and compared to the traditional quantification strategies. Moreover, the validity of the newly adopted approach has been verified by the targeted profiling of multiple biologically active endogenous steroids in more than 500 samples of mouse plasma in total. SignificanceUnderestimation of hurdles associated with steroid analysis often compromises the accurate steroid quantification. Our comprehensive, fully validated UHPLC-MS/MS method targeting a wide spectrum of endogenous steroids, mitigating steroid crosstalk and using a minimal sample volume together with a novel surrogate matrix-background subtraction approach significantly advances steroid analysis for research and clinical applications covering multiple biological scopes.

Separation of no-carrier-added Bi and stable Bi from thallium

Abstract No carrier added 204,206Bi radioisotopes were produced by alpha induced reaction on Tl2CO3 target. Liquid liquid extraction method using 18-crown-6 dissolved in nitrobenzene and HClO4 was developed for the separation of NCA 204,206Bi from bulk Tl target. Bulk Tl was observed to be extracted by the organic phase at higher HClO4 concentrations leaving NCA Bi radioisotopes in the aqueous phase. At 0.01 M 18-crown-6 concentration with 2 M HClO4, separation factor (S Tl/Bi) as high as 3.7 × 103 was achieved. The separation experiment was repeated with stable isotopes of Bi and Tl. The extent of separation was monitored by ICP-OES and the results corroborated with radiometric methods.

Improved and Novel Methods for Investigating Organophosphate Esters in Particulate Matter

A pressurized liquid extraction (PLE) method for the extraction of 31 organophosphate esters (OPEs) and novel organophosphate esters (NOPEs) has been developed. Unlike previously published methods, this method utilizes the high-throughput nature of PLE (as opposed to Soxhlet or sonication methods) without using potentially harmful organic solvents like methylene chloride. Combinations of hexane and acetone and hexane and ethyl acetate at various temperatures were examined. Extracts were concentrated and analyzed via gas chromatography–mass spectrometry. The final optimized method utilized 1:1 v/v hexane/ethyl acetate at 100 °C for three static cycles (5 min each) at 80% flush volume and a 100 s N2 purge. This provided average surrogate corrected target analyte percent recoveries in spike and recovery experiments (n = 6) for OPEs and NOPEs of 106 ± 13%, with average surrogate recoveries of 88.6 ± 7.3%. The developed method was further validated using standard reference materials and was then applied to atmospheric particulate matter samples collected in the city of Providence, RI. The dataset reflected ambient concentrations of 16 OPEs and NOPEs (reported in pg m−3) for the first time in the greater Providence metropolitan area, including one of the first reports of NOPEs in atmospheric particulate matter in the U.S.

Applications of Sample Preparation Techniques in the Analysis of New Psychoactive Substances

The global rise of new psychoactive substances (NPSs) poses challenges for their analysis in biological matrices due to their complex chemistries and short market lifespan. A comparative study for the simultaneous extraction, separation, and detection of 19 NPSs was conducted. Six solid-phase extraction (SPE) methods and one supported liquid extraction method (SLE) were compared for the extraction of analytes from blood, serum, plasma, and urine. Comparisons of four derivatization agents were conducted, at four temperatures and two incubation times. Extraction methods were assessed by precision, sensitivity, and extraction efficiency. Derivatizing agents were assessed on their selectivity and sensitivity, and a three-way ANOVA was conducted to determine statistical significance. CSDAU SPE cartridges were shown to be the most efficient when extracting analytes from blood, serum, and plasma, whereas Xcel I cartridges performed the strongest when extracting analytes from urine. SPE extraction efficiencies, when utilizing the best-performing cartridges, ranged from 49 to 119%. SLE successfully extracted all analytes from all matrices (ranging from 22 to 120%). Pentafluoropropionic anhydride: ethyl acetate was the most successful derivatizing agent, allowing all analytes to be detected, with the highest peak area responses and more unique spectra. The optimum temperature for incubation was 37 °C, with no statistical difference found between the two incubation times.

Liquid–liquid extraction method for the gas chromatography – mass spectrometry analysis of volatile fatty acids in wastewater

ABSTRACT This study addresses the need to transition WWTPs from energy-intensive operations to carbon-neutral and energy-efficient systems by examining VFAs’ concentrations, which vary significantly with different types of wastewater. The analytical performance of the liquid–liquid extraction (LLE) method using two solvents – methyl-tert-butyl ether (MTBE) and dichloromethane (DCM) – followed by injection into a gas chromatography-mass spectrometry (GC-MS) system is evaluated. The limit of quantification (LOQ) and limit of detection (LOD) for VFAs ranged from 3 to 7.41 mg/L and 0.91 to 2.25 mg/L, respectively. Precision for lower VFAs (ethanoic (C2), propanoic (C3), 2-methyl-propanoic (iC4), butanoic (C4), methyl-butanoic (iC5), and pentanoic acids (C5)) using DCM and MTBE ranged from 1.99% to 8.64% and 1.21% to 6.68%, respectively, with accuracies of 90.35% to 107.27% and 81.55% to 105.96%, respectively. For higher VFAs (iC6, C6, and C7) using DCM, precision ranged from 18.44% to 27.06%, and accuracy ranged from 70.1% to 101.4%. In contrast, MTBE failed to detect VFAs iC6, C6, and C7. These findings underscore the importance of solvent selection in VFA analysis and its implications for optimising WWTP operations.

Associations between neonicotinoid insecticide levels in follicular fluid and serum and reproductive outcomes among women undergoing assisted reproductive technology: An observational study

Neonicotinoid insecticides (NEOs) are a widely used type of insecticide found globally, leading to broad human exposure. However, there is limited research on how internal exposure levels of NEOs and their metabolites impact in vitro fertilization/intracytoplasmic sperm injection (IVF/ICSI) outcomes. A study was conducted at the Sixth Affiliated Hospital of Sun Yat-sen University between 2017 and 2020 involving 436 women undergoing IVF/ICSI treatment. Data on demographics and clinical history were collected from medical records. The concentrations of 11 NEOs and 4 NEO metabolites in follicular fluid and serum were measured using a salting-out assisted liquid–liquid extraction method and liquid chromatography–tandem mass spectrometry. Our findings indicated that NEOs were prevalent in women with infertility. One NEO metabolite, N-dm-ACE, was detected in all samples with median concentrations of 0.221 ng/mL in follicular fluid and 0.228 ng/mL in serum. The study showed a decrease in the number of retrieved oocytes, mature oocytes, 2 PN zygotes, and high-quality embryos as the number of exposed NEOs in follicular fluid increased. Women in the highest tertile of N-dm-ACE exposure had fewer mature oocytes, 2 PN zygotes, and lower oocyte maturity rates compared to those in the lowest tertile. The findings suggest that exposure to NEOs may negatively impact reproductive outcomes in IVF/ICSI pregnancies, particularly affecting oocyte retrieval and embryo quality. This study highlights the potential adverse effects of environmental NEO exposure on IVF/ICSI outcomes, emphasizing the importance of considering such exposures in preconception care.

2-nitro-4-nonylphenol-based extractant for selective extraction of lithium from carbonate precipitation mother liquors

In this work, for the first time we proposed a mixture based on 2-nitro-4-nonylphenol as a lithium-selective binary extractant, in which the nitro group simultaneously participates in the formation of a six-membered metallocycle and increases the acidity of the phenolic group. The extraction of alkali metals (Li, Na, K) by a mixture of 2-nitro-4-nonylphenol and trioctylphosphinoxide in dodecane was studied in detail. The extraction of Li from mother liquors after Li2CO3 precipitation was considered as a practical application of the new binary extractant. It was shown that by using only liquid extraction methods, a high degree of concentration and purification of final product can be achieved. Mother liquor of Li2CO3 precipitation was concentrated by Li more than 50 times. Degree of lithium concentrate purification from Na and K was more than 5500 and 100,000 times, correspondingly.

A practical approach to supported liquid extraction and measurement of 18 steroids in plasma and serum by targeted liquid chromatography tandem mass spectrometry

Chromatography combined with mass spectrometry is a gold standard technique for steroid measurement, however the type of sample preparation, the dynamic range and reliability of the calibration curve, the chromatographic separation and mass spectrometry settings ultimately determine the success of the method. The steroid biosynthetic pathway is conserved in higher mammals and literature demonstrates that the concentration ranges of different steroid groups are relatively comparable across species. We sought to develop a robust and reliable multi steroid targeted analysis method for blood that would have wide application across higher mammals. The method was developed following bioanalytical method validation guidelines to standards typically applied to human clinical studies, including isotopically labelled internal standards where at all possible. Here we describe the practical approach to a 96-well supported liquid extraction (SLE) method of extraction from plasma (200 µL) using an Extrahera liquid handling robot (Biotage, Sweden), including quality control samples, followed by a comprehensive separation and targeted LC-MS/MS analysis of 18 steroids in plasma (pregnenolone, progesterone, 17α-hydroxyprogesterone, 11-deoxycorticosterone, corticosterone, 11-dehydrocorticosterone, aldosterone, 11-deoxycortisol, 21-deoxycortisol, cortisol, cortisone, androstenedione, testosterone, 5α-dihydrotestosterone, dehydroepiandrosterone, estrone, 17β-estradiol and estriol).•SLE in a 96-well format of up to 74 biological plasma samples, enriched with multiple isotopically labelled internal standards, a 12-point aqueous calibration curve, and 6 serum quality controls, designed to monitor long-term performance of the method•Chromatographic separation of multiple steroids along the gradient, with ammonium fluoride mobile phase additive to improve sensitivity, followed by electrospray ionisation and constant polarity switching•Aqueous calibration standards that cover physiologically relevant ranges - high nanomolar glucocorticoids, low nanomolar androgens and picomolar ranges for estrogens and steroid intermediates.

Candidate reference measurement procedure for serum 17‐hydroxyprogesterone quantification via isotope dilution liquid chromatography–tandem mass spectrometry

AbstractBackgroundAccurate quantification of 17‐hydroxyprogesterone (17‐OHP) in serum is vital for clinical and research applications. However, inter‐laboratory variability in test results exists owing to the lack of a standardized reference measurement procedure (RMP). Therefore, in this study, we developed a highly accurate, cost‐effective, and user‐friendly candidate RMP (cRMP) for analyzing 17‐OHP in serum.MethodsWe quantified 17‐OHP in serum using a one‐step liquid–liquid extraction method with the addition of 17‐OHP‐13C3, followed by liquid chromatography–tandem mass spectrometry. The ability of these methods to suppress interference was evaluated by chromatographic analysis. We assessed accuracy, specificity, the lower limit of quantitation, linearity, and matrix effects by following the standards specified by the Clinical and Laboratory Standards Institute. The consistency between the developed cRMP and the chemiluminescence method was evaluated through experiments with 120 clinical samples.ResultsThe developed cRMP required only 8 min for accurate quantification of serum 17‐OHP without bias from matrix effects or interference from 19 metabolites added as potential interferents. The method exhibited favorable measurement performance, with a quantitation limit of 0.086 ng/mL, linear range of 0.1–400 ng/mL, a total imprecision of ≤2.90%, spike recovery of 100.1%–100.6%, and relative deviations from assigned target values (RfB Institution) of −2.91% to 1.10%. The cRMP demonstrated good consistency with the conventional assay (chemiluminescence method), with a correlation coefficient R of 0.96977.ConclusionA cRMP with high accuracy, cost‐effectiveness, and convenient operation was developed for quantifying 17‐OHP in serum. Its simplicity and robust performance make it an invaluable addition to the arsenal of analytical tools available for laboratories. This method can enhance the accuracy and reliability of 17‐OHP measurements across various laboratories.

Quantification of Irgafos P-168 and Degradative Profile in Samples of a Polypropylene/Polyethylene Composite Using Microwave, Ultrasound and Soxhlet Extraction Techniques

In polypropylene/polyethylene composite (C-PP/PE) production, stabilizing additives such as Irgafos P-168 are essential as antioxidant agents. In this study, an investigation was carried out that covers different solid–liquid extraction methods (Soxhlet, ultrasound, and microwaves); various variables were evaluated, such as temperature, extraction time, the choice of solvents, and the type of C-PP/PE used, and the gas chromatography coupled to mass spectrometry (GC-MS) technique was used to quantify the presence of Irgafos P-168 in the C-PP/PE samples. The results revealed that microwave extraction was the most effective in recovering Irgafos P-168. A recovery of 96.7% was achieved when using dichloromethane as a solvent, and 92.83% was achieved when using limonene as a solvent. The ultrasound technique recovered 91.74% using dichloromethane and 89.71% using limonene. The Soxhlet extraction method showed the lowest recovery percentages of 57.39% using dichloromethane as a solvent and 55.76% with limonene, especially when the C-PP/PE was in the form of pellets. The degradation products that obtained the highest degradation percentages were Bis (di-test-butyl phenyl) phosphate and Mono (di-test-butyl phenyl) phosphate using the microwave method with dichloromethane as a solvent and PP in film. Finally, the possible mechanisms for forming the degradation compounds of Irgafos P-168 were postulated.

Bioanalytical method development and validation for quantification of amivantamab in rat plasma by LC-MS/MS

BackgroundAmivantamab is a monoclonal bispecific anti-EGFR-MET antibody used to treat non-small cell lung cancer. There were no published methods using a liquid chromatographic—tandem mass spectrometric approach to develop and validate a feasible, novel, and thoroughly validated method for quantifying amivantamab in rat plasma.ResultsThe liquid–liquid extraction method was used to extract the analyte from rat plasma. The analyte was separated using acetonitrile–ammonium formate buffer (40:60) as a mobile phase on waters, alliance e-2695 model high-pressure liquid chromatographic system having Agilent eclipse C18, 150 mm × 4.6 mm, 3.5 µm column. The overall runtime was 6 min at a 1.0 ml/min flow rate. The method showed significant sensitivity and acceptable linearity over the 5.00–100.00 ng/ml concentration range. Accuracy was proved by mean percent recovery ranging from 98.03 to 99.99%. The intraday precision coefficient of variation (%) ranged between 0.31 and 5.43. Also, the findings such as Cmax, tmax, AUC0− t, AUC0− ∞, and half-life values of amivantamab showed that the technique was helpful for pharmacokinetic studies.ConclusionsAll the validated parameters were found to be within the acceptable range. The validated method was found to be simple, accurate, precise, and reproducible and hence can be used for the routine analysis of amivantamab, such as in-process quality control by liquid chromatographic—tandem mass spectrometry.

An integrated method for rapid extraction of fluorescent whitening agents from selected cosmetics by in situ formation of deep eutectic solvent

A novel extraction methodology was developed based on deep eutectic solvent (DES) in situ formation. The solvent was synthesized from a binary mixture of L-cysteine, functioning as a hydrogen bond acceptor, and 2-methylphenol, serving as a hydrogen bond donor. The DES’s inherent molecular structures and extensive hydrogen bonding networks were characterized using the Fourier-transform infrared spectroscopy (FT-IR), while its hydrophobic nature was assessed by determining molecular polarity. Its extraction efficiency was demonstrated through the extraction of fluorescent whitening agents (FWAs) in cosmetic products, acting as a model analytical application. This was accomplished using vortex-assisted emulsification solid–liquid extraction (SLE) method, followed by high-performance liquid chromatography-fluorescence detection. Response surface methodology was employed to optimize extraction conditions in a multivariate experimental design. This approach streamlined the multi-operation extraction process via ingeniously integrating extraction and clean-up into a single step, resulting in significant reductions in extraction time required and high sample throughputs of approximately 40 samples per hour. The methodology was validated and exhibited excellent linearity in concentration ranges of 0.01–24 mg/L for five FWAs and 0.01–40 mg/L for other three FWAs, with correlation coefficients (r) ranging from 0.9985 to 1.000. The limits of detection and quantification were in the range of 0.03–0.26 mg kg−1 and 0.10–0.87 mg kg−1, respectively. The reliability and practicality of the proposed method were affirmed by quantifying eight FWAs in ninety-four commercially available facial masks and whitening creams, yielding recoveries values between 90.0 % and 106.0 % with relative standard deviations (RSDs) of 1.0–4.3 %. Inorganic ions and organic compounds present in the samples had minimal impact on FWAs detection following sample pre-treatment. This procedure showcased exceptional extraction capabilities towards a diverse array of FWAs with the aid of multiple interactions, suggesting significant potential for increasing sample throughput while reducing organic solvent and material consumptions compared with conventional SLE methods. The low-toxicity DES is an excellent alternative to traditional extractants typically applied to SLE techniques.

Development of an Analytical Method For Determination of Urine 3-Phenylpyruvic Acid Based on Liquid-Liquid Extraction and LC-MS/MS

Aim: The aim of this study is to develop a rapid, precise, specific LC MS MS method for the determination of 3-phenylpyruvic acid, which has an important place in the diagnosis of phenylketonuria, a metabolic disease resulting from Phenylalanine Hydroxylase Enzyme deficiency.
 Materials and Methods : Analytical measurements were made with Acqutiy UPLC MS MS (Waters Xevo TQD). The chromatographic separation was operated on an Acquity UPLC Phenyl column (50 mm × 2.1 mm, 1.7 μm) with gradient elutionusing 0.1% formic acid containing water and methanol as the mobile phase. Within the scope of the study, firstly, sample preparation steps were focused and dispersive liquid liquid extraction and traditional liquid extraction methods were examined. The best results were obtained in the conventional liquid liquid extraction method, in which dichloromethane was used as the extraction solvent. In addition, in this study, trans cinnamic acid was tested as an internal standard for the determination of 3-phenylpyruvic acid and passed the validation steps.
 Results : The linear range of the developed LC MS MS method was found to be between 0.009-5 M, while the detection limit was found to be 0.001 M. Intraday repeatability was below 7% for 3 levels, and interday repeatability was below 10%. In the recovery trial, which showed the accuracy of the method, the results in the urine sample for 3 levels were in the range of 97%-103%, and there was no significant ion suppression in the matrix effect trial, which showed how clean the final matrix obtained as a result of the sample preparation steps was.
 Conclusion: As a result, a fast, inexpensive LC MS MS method has been developed for 3-Phenylpyruvic acid.

Method Development and Validation in Water Matrix Employing Tandem Mass Spectrometry: Quantitative Analysis of 76 Multiclass Pesticides in Groundwater Samples Collected from Delhi Ncr Region by Quechers Based Liquid-liquid Extraction Method

A miniaturized, QuEChERS based, liquid–liquid extraction method followed by tandem gas chromatography–mass spectrometry determination was developed and validated for 76 pesticide residues determination in water using European SANTE/11312/2021 guideline and monitored the 70 ground water samples collected from Delhi NCR, India region for the determination of pesticide residues. The accuracy, precision, specificity, linearity, recovery, repeatability, reproducibility, robustness, limit of detection and limit of quantification of the method were evaluated. Uncertainty measurement was calculated for each analyte. The samples were extracted with dichloromethane using liquid-liquid extraction process. Each Pesticide was optimized in terms of different MS parameters and chromatographic conditions by GC-MS/MS using Multiple Reaction Monitoring (MRM) mode. In linearity regression co-efficient (R2) value of each pesticide was determined in the range of 0.9856-0.9997. The percent average recoveries were found from 87.98—119.99 at 1, 5 and 10 LOQ spiking level. The method performance complied with the regulatory requirements, and thus, can be implemented. LOD and LOQ of the pesticides were found 10µg/L and 30µg/L respectively. Expanded Measurement of uncertainty of all pesticides was below ±50 percent of mean recovery value as per SANTE 11312/2021. Organophosphorous, fungicides, and pyrethroids were the group of pesticides most frequently found. In this study, 12 pesticides were found above the MRL (EEC Council Directive 1980/778/EEC). Additionally, dieldrin, which is now banned by law in India, was found in samples of ground water. The method provided a high throughput analysis of multi-class pesticides with satisfactory selectivity, sensitivity, accuracy, and precision.

Evaluation of the Health Risk and Distribution Characteristics of Pesticides in Shallow Groundwater, South Korea

In this work, a method of simultaneously analyzing pesticide concentration and assessing its risks was developed. Assessments were conducted to evaluate the distribution characteristics and risks to human health of pesticides in shallow groundwater in agricultural areas. We developed multi-residue analytical methods using liquid chromatography (LC-MS/MS) and gas chromatography–tandem mass spectrometry (GC-MS/MS) to analyze 57 pesticides in groundwater. In addition, risk assessments were performed by setting scenarios considering the routes of pesticide infiltration into groundwater. For the simultaneous analysis of 57 pesticides, the liquid–liquid extraction method was applied twice using dichloromethane under acidic and alkaline conditions. The extract was concentrated and analyzed using LC-MS/MS (41 pesticides) and GC-MS/MS (16 pesticides). The precision and accuracy ranges of the analytical methods were 0.1~12.9% (within ±15%) and 80.3~113.6% (within ±20%), respectively. The limit of quantification was found to range from 0.0004 to 0.0677 μg/L. In total, 57 pesticides were monitored in 200 groundwater wells from 2019 to 2020. Twenty-six pesticides, including metolachlor and imidacloprid, were detected, with an average concentration of 0.0008 μg/L in groundwater. The pesticide types and detection levels differed depending on the survey period and surrounding land. When the risks associated with alachlor, metolachlor, and carbofuran were assessed, their health risks when found in groundwater were evaluated to be negligible (non-carcinogenic risk: less than 10−3, carcinogenic risk: less than 10−6).

Effective removal of personal care product residues from aqueous media using hydrophobic deep eutectic solvents: Experimental and computational approach

Personal care product (PCP) residues - classified under micropollutants (MPs)- are widely found in aquatic environments, posing trace-level toxicity. Traditional water treatment techniques struggle to remove these toxins effectively. Deep eutectic solvents (DESs), the liquid mixtures typically composed of hydrogen bond donors (HBDs) and hydrogen bond acceptors (HBAs), have recently emerged as a viable alternative for extracting pollutants from water. Among DESs, hydrophobic deep eutectic solvents (HDESs) exhibit low water miscibility and unique solvent properties. The main objective of this study is to synthesize HDESs to effectively eliminate 2-naphthol and methylparaben- two of the significant chemical contaminants in PCPs- from aqueous media. HDESs were prepared by mixing different terpenes (menthol and thymol) and long-chain carboxylic acids at varying molar ratios. They were characterized using different spectroscopic and thermal techniques. The density and viscosity of the pure DESs were measured as afunction of temperature. Experimental studies were carried out using the liquid–liquid extraction (LLE) method, and the factors influencing the efficiency of extraction were optimized.Considering the limited number of studies on the extraction mechanism of MPs from aqueous media, this study employs comprehensive computational methods, including density functional theory (DFT) and the COnductor-like Screening MOdel for Real Solvents (COSMO-RS), to provide a detailed interpretation of the extraction mechanism. A series of successive extractions were conducted to reduce the DES usage to ensure economic viability. The reusability of the best-performed DES was explored. Additionally, the regeneration of one of the DESs was accomplished through activated carbon-based recovery.---------------------------------------------------------------------------------------------------------------------

Profiling and evaluation of phenolic compounds in olive mill wastewater in Jordan

Abstract Phenolic compounds (PCs) are prevalent in olive mill wastewater (OMW), offering numerous health benefits but concurrently posing environmental challenges. This study aims to comprehensively characterize PCs in OMW, both qualitatively and quantitatively. An accurate, sensitive, and cost-effective method was successfully developed for extracting and quantifying seven PCs in OMW. The extraction procedure was optimized to achieve the maximum recovery using a liquid-liquid extraction method. Concentrations of the identified PCs were determined using a high-performance liquid chromatography-diode array detector (HPLC-DAD). The seven PCs peaks were successfully separated on an RP-C8 column within a 23-minute runtime using a gradient mobile phase. The method underwent thorough validation, producing satisfactory results. Subsequently, the developed method was applied to analyze OMW from four olive mills in Jordan, revealing PC concentrations ranging from 139 to 430 mg/L. Tyrosol and hydroxytyrosol were identified as the most abundant compounds. Additionally, gas chromatography-mass spectrometry (GC-MS) separated and identified forty PCs. The total phenolic content was quantified, reaching a value of 1839 mg/L. Moreover, the antioxidant activity was assessed, yielding a maximum value of 95.8%. These results underscore the substantial levels of PCs in OMW, highlighting the importance of economically utilizing this water.